CN102704323B - Bamboo reed dissolving pulp pretreating method - Google Patents
Bamboo reed dissolving pulp pretreating method Download PDFInfo
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- CN102704323B CN102704323B CN201210221917.5A CN201210221917A CN102704323B CN 102704323 B CN102704323 B CN 102704323B CN 201210221917 A CN201210221917 A CN 201210221917A CN 102704323 B CN102704323 B CN 102704323B
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Abstract
The invention provides a bamboo reed dissolving pulp pretreating method, which comprises the following steps of: (1) adding bamboo reed sheets into hydrolysis solution, and soaking in a solid acid catalyst; (2) cooking all the materials in the step (3) at temperature of 130-150 DEG C for 30-60 minutes; (3) raising the temperature to 160-180 DEG C, and continuously keeping the temperature for 30-60 minutes; (4) respectively collecting the cooked pulp and the solid acid catalyst, and washing the cooked pulp with water with the temperature of 80-90 DEG C; (5) adding sodium hydroxide solution into the cooked pulp, soaking, cooking, and collecting the cooked pulp for two times; and (6) adding sodium thiosulfate and hydrogen dioxide solution into the pulp cooked for two times, then adding water and bleaching, thus obtaining bamboo reed dissolving pulp. With the method, the economic value of the bamboo reed can be fully played, the investment is small, and the process is simple. The pretreating method is especially suitable for pretreating technology at bamboo reed producing places, and a raw material is increased for papermaking, cotton spinning and building materials.
Description
Technical field
The present invention relates to the preliminary working technology that giantreed produces comprehensive utilization.
Background technology
Giantreed is widely distributed in China, North gets Liaoning, reaches Guangxi in the south, and producing maximum is riverine sea wall band, and to administering environment and the anti-landslide face of flood control, giantreed has been brought into play unique effect.Giantreed growth is simultaneously fast, and adaptive capacity is very strong, is also easy to breeding, has good economic worth.But owing to being subject to impact and the restriction of the many factors such as environmental protection and economic development imbalance, China is also in the low-level stage in the comprehensive utilization of giantreed, a large amount of giantreeds can only be used as fuel, does not bring into play due economic worth.Therefore utilize environment and the geography of giantreed growth, improve the economic worth of giantreed comprehensive utilization, give full play to gather materials on the spot, reduce costs, a major issue that protection of the environment is giantreed process technology.
Summary of the invention
The object of this invention is to provide a kind of giantreed dissolving pulp preliminary working method, for overcoming the defect of prior art.
Method of the present invention, comprises the steps:
(1) a crushes giantreed, pulverizes segment, and length is 3 ~ 5cm;
(2) b, by the washing of giantreed tablet, removes plaster dirt, dress pot;
(3) c adds hydrating solution by giantreed sheet, in solid acid catalyst, soaks 30-60 minute, and hydrating solution weight is 1.5～2: 1 with the ratio of giantreed tablet weight;
The weight consumption of solid acid catalyst is 5～15% of giantreed tablet;
The parts by weight of described hydrating solution comprise:
Described solid acid catalyst is SO
4 2--ZrO
2type solid acid catalyst, is comprised of the element sulphur of more than 90% zirconium dioxide and 0.1～0.5% platinum and 0.5～5%, and average grain diameter is 20 nanometers, and by being processed into agglomeration sphere-like, sphere diameter is 4～6mm conventionally.
Preparation by the following method:
By ZrOCl
2with the ammoniacal liquor of weight concentration 25%, at 50 ℃, be hydrolyzed 2 hours (PH is controlled at 10), generate after zirconium hydroxide, use again 90 ℃ of deionized water soaking and washing 10 hours, then filter, then with the cleanings of 90 ℃ of deionized waters, after refiltering, at 110 ℃, be dried 10 hours, roasting 5 hours at 680 ℃, then with soaking 3 hours in the sulfuric acid of weight concentration 1% and the ammonium chloroplatinate mixed liquor of weight concentration 1.67%, at 110 ℃, be dried 3 hours, roasting 4 hours at 680 ℃ again, makes solid super-strong acid.(referring to Teaching Materials at College level < < chemical functional materials outline > > mono-book)
The solid acid catalyst that the present invention uses is selected from the SO of the positive big vast biodiesel equipment of Wuxi City Science and Technology Ltd.
4 2--ZrO
2type solid acid catalyst.
(4) d is then by whole materials of step (3), at the temperature of 130 ℃-150 ℃, and boiling 30-60 minute;
(5) e is warming up to 160 ℃-180 ℃, continues to keep 30-60 minute;
(6) f venting, collects respectively boiling slurry and solid acid catalyst, and boiling slurry cleans with the water of 80-90 ℃;
(7) g is in boiling slurry, and adding weight concentration is 5-10% sodium hydroxide solution, soaks 30-60 minute, and then boiling 30-60 minute at 130 ℃-150 ℃, collects 2 times boiling slurry;
The weight consumption of described sodium hydroxide solution, in NaOH, is 5～6% of raw material giantreed tablet;
(8) h adds boiling slurry 2 times by sodium thiosulfate and hydrogenperoxide steam generator, then adds water to slurry and flood, and passes into steam, is warming up to 90 ℃-120 ℃, and bleaching 30-60 minute collects bleaching slurry; For the giantreed dissolving pulp of preliminary working;
The weight consumption of component is:
Raw material giantreed tablet: sodium thiosulfate=1:0.05～0.15;
Raw material giantreed tablet: weight concentration 30% hydrogen peroxide=1:0.2～0.4
Described giantreed dissolving pulp, can be for the preparation of cellulose ether or paper making raw material.
The invention has the advantages that and utilized resourceful giantreed for raw material, improve preliminary working technology, give full play to the economic worth of giantreed; Changed the traditional handicraft that existing dissolving pulp is produced; introduce solid acid catalysis agent method and carry out prehydrolysis and degradation of hemicellulose; the useless composition such as lignin, glycan; significantly improved chemically treated ability; especially reduce the corrosion to production equipment, reduced energy resource consumption, significantly reduced the black liquor producing in dissolving pulp production process; improved the effective utilization to water resource, protection of the environment particular significant effect.The present invention invests little, and technique is simple, is particularly suitable for the preliminary working technology in the giantreed place of production, for papermaking, cotton spinning, construction material have increased new raw material.
The specific embodiment
Solid acid catalyst is SO
4 2--ZrO
2type solid acid catalyst, is comprised of the element sulphur of more than 90% zirconium dioxide and 0.1～0.5% platinum and 0.5～5%, and average grain diameter is 20 nanometers, and by being processed into agglomeration sphere-like, sphere diameter is 4～6mm conventionally.
Preparation by the following method:
By ZrOCl
2with 25% ammoniacal liquor, at 50 ℃, be hydrolyzed 2 hours (PH is controlled at 10), generate after zirconium hydroxide, use again 90 ℃ of deionized water soaking and washing 10 hours, then filter, then with the cleanings of 90 ℃ of deionized waters, after refiltering, at 110 ℃, be dried 10 hours, roasting 5 hours at 680 ℃, then soak 3 hours with being mixed with in 1% dilute sulfuric acid and 1.67% ammonium chloroplatinate mixed liquor, at 110 ℃ dry 3 hours, roasting 4 hours at 680 ℃ again, makes solid super-strong acid.
Embodiment 1
(a) giantreed is crushed, pulverize segment, average length is 3cm;
(b) by the washing of giantreed tablet, remove plaster dirt, dress pot;
(c) giantreed sheet is added to hydrating solution, in solid acid catalyst, soak 30 minutes, hydrating solution weight is 1.5: 1 with the ratio of giantreed tablet weight;
The weight consumption of solid acid catalyst is 5% of giantreed tablet;
The parts by weight of described hydrating solution comprise:
(d) then by whole materials of step (3), at 130 ℃, boiling 30 minutes;
(e) be warming up at 160 ℃ and continue to keep 30 minutes;
(f) venting, collects respectively boiling slurry and solid acid catalyst, and boiling slurry cleans with the water of 80-90 ℃;
(g) in boiling slurry, adding weight concentration is 5% sodium hydroxide solution, soaks 30 minutes, and then, at 130 ℃, boiling 30 minutes, collects 2 times boiling slurry;
The weight consumption of sodium hydroxide solution, in NaOH, is 5% of raw material giantreed tablet;
(h) sodium thiosulfate and hydrogenperoxide steam generator are added to boiling slurry 2 times, then add water to slurry and flood, pass into steam, be warming up to 90 ℃ ℃, bleach 30 minutes, collect bleaching slurry; For the giantreed dissolving pulp of preliminary working;
The weight consumption of component is:
Raw material giantreed tablet: sodium thiosulfate=1:0.05.
Raw material giantreed tablet: 30% hydrogen peroxide=1:0.2.
Embodiment 2
(a) giantreed is crushed, pulverize segment, average length is 5cm;
(b) by the washing of giantreed tablet, remove plaster dirt, dress pot;
(c) giantreed sheet is added to hydrating solution, in solid acid catalyst, soak 60 minutes, hydrating solution weight is 2: 1 with the ratio of giantreed tablet weight;
The weight consumption of solid acid catalyst is 15% of giantreed tablet;
The parts by weight of described hydrating solution comprise:
(d) then by whole materials of step (3), at 150 ℃, boiling 60 minutes;
(e) be warming up to 180 ℃, continue to keep 60 minutes;
(f) venting, collects respectively boiling slurry and solid acid catalyst, and boiling slurry cleans with the water of 80-90 ℃;
(g) in boiling slurry, adding weight concentration is 10% sodium hydroxide solution, soaks 60 minutes, and then 150 ℃, boiling 30 minutes, collects 2 times boiling slurry;
The weight consumption of sodium hydroxide solution, in NaOH, is 6% of raw material giantreed tablet;
(h) sodium thiosulfate and hydrogenperoxide steam generator are added to boiling slurry 2 times, then add water to slurry and flood, pass into steam, be warming up to 120 ℃, bleach 60 minutes, collect bleaching slurry; For the giantreed dissolving pulp of preliminary working;
The weight consumption of component is:
Raw material giantreed tablet: sodium thiosulfate=1:0.1;
Raw material giantreed tablet: 30% hydrogen peroxide=1:0.4.
Embodiment 3
(a) giantreed is crushed, pulverize segment, average length is 4cm;
(b) by the washing of giantreed tablet, remove plaster dirt, dress pot;
(c) giantreed sheet is added to hydrating solution, in solid acid catalyst, soak 50 minutes, hydrating solution weight is 1.75: 1 with the ratio of giantreed tablet weight;
The weight consumption of solid acid catalyst is 10% of giantreed tablet;
The parts by weight of described hydrating solution comprise:
(d) then by whole materials of step (3), at 140 ℃, boiling 45 minutes;
(e) be warming up at 170 ℃ and continue to keep 50 minutes;
(f) venting decompression, collects respectively boiling slurry and solid acid catalyst, and boiling slurry cleans with the water of 80-90 ℃;
(g) in boiling slurry, adding weight concentration is 8% sodium hydroxide solution, soaks 45 minutes, and then 140 ℃, boiling 45 minutes, collects 2 times boiling slurry;
The weight consumption of sodium hydroxide solution, in NaOH, is 5.5% of raw material giantreed tablet;
(h) sodium thiosulfate and hydrogenperoxide steam generator are added to boiling slurry 2 times, then add water to slurry and flood, pass into steam, be warming up to 105 ℃, bleach 45 minutes, collect bleaching slurry; For the giantreed dissolving pulp of preliminary working;
The weight consumption of component is:
Raw material giantreed tablet: sodium thiosulfate=1:0.15,
Raw material giantreed tablet: 30% hydrogen peroxide=1:0.3.
Embodiment 4
Adopt bioassay standard and institution of higher education's specialized teaching material (Plant Fiber Chemistry, Yang Shuhui chief editor) book recommend method of GB/T 744-1989 paper pulp alpha-cellulose to detect, result is as follows:
From embodiment data determination effect of the present invention, be better than CN20110211009.3, and work simplification, sulfate consumption are few.
Claims (4)
1. giantreed dissolving pulp preliminary working method, is characterized in that, comprises the steps:
(1) giantreed sheet is added to hydrating solution, in solid acid catalyst, soak;
(2) then by whole materials of step (3), at the temperature of 130 ℃-150 ℃, boiling 30-60 minute;
(3) be warming up to 160 ℃-180 ℃, continue to keep 30-60 minute;
(4) collect respectively boiling slurry and solid acid catalyst, boiling slurry cleans with the water of 80-90 ℃;
(5) in boiling slurry, add sodium hydroxide solution, soak, then boiling, collects 2 times boiling slurry;
(6) sodium thiosulfate and hydrogenperoxide steam generator are added to boiling slurry 2 times, then add water, bleaching, obtains described giantreed dissolving pulp;
Described solid acid catalyst is SO
4 2--ZrO
2type solid acid catalyst, is comprised of the element sulphur of more than 90% zirconium dioxide and 0.1～0.5% platinum and 0.5～5%, and average grain diameter is 20 nanometers, and by being processed into agglomeration sphere-like, sphere diameter is 4～6mm.
2. method according to claim 1, is characterized in that, hydrating solution weight is 1.5～2: 1 with the ratio of giantreed tablet weight;
The weight consumption of solid acid catalyst is 5～15% of giantreed tablet;
The parts by weight of described hydrating solution comprise:
3. method according to claim 1, is characterized in that, in step (5), in boiling slurry, adding weight concentration is 5-10% sodium hydroxide solution, soaks, and then boiling 30-60 minute at 130 ℃-150 ℃, collects 2 times boiling slurry; The weight consumption of described sodium hydroxide solution, in NaOH, is 5～6% of raw material giantreed tablet.
4. method according to claim 1, it is characterized in that, in step (6), sodium thiosulfate and hydrogenperoxide steam generator are added to boiling slurry 2 times, add again water, 90 ℃ of-120 ℃ of bleachings, obtain giantreed dissolving pulp, and the weight consumption of component is: raw material giantreed tablet: sodium thiosulfate=1:0.05～0.15; Raw material giantreed tablet: weight concentration 30% hydrogen peroxide=1:0.2～0.4.
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| CN201210221917.5A CN102704323B (en) | 2012-06-29 | 2012-06-29 | Bamboo reed dissolving pulp pretreating method |
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| CN201210221917.5A CN102704323B (en) | 2012-06-29 | 2012-06-29 | Bamboo reed dissolving pulp pretreating method |
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| CN102704323A CN102704323A (en) | 2012-10-03 |
| CN102704323B true CN102704323B (en) | 2014-04-16 |
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| CN102424437B (en) * | 2011-09-07 | 2013-06-26 | 宜宾丝丽雅集团有限公司 | Method for treating prehydrolysis liquid of bamboo dissolving pulp |
| CN102352572B (en) * | 2011-09-30 | 2013-07-24 | 重庆理文造纸有限公司 | Preparation method for bamboo wood dissolving pulp |
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